Unexpected differences in the reactivity between MPh2Cl2 (M=Pb or Sn) and Benzil (cas 134-81-6) bis(thiosemicarbazone). X-ray crystal structure of Benzil (cas 134-81-6) bis(thiosemicarbazonate)lead(II)

Add time:10/01/2019    Source:infona.pl

The differences in the reactivity of diphenyllead and diphenyltin dichloride with Benzil (cas 134-81-6) bis(thiosemicarbazone) LH 6 are explored. The reaction of PbPh 2 Cl 2 afforded the complex [Pb(LH 4 )] 1, containing the ligand doubly deprotonated and without the phenyl groups bonded to the metal. The reaction with SnPh 2 Cl 2 in the absence of solvent yielded the complex [Sn(LH 4 )Cl 2 ] 2. The lead(II) complex, also obtained by the reaction with lead(II) nitrate, was formed by a redistribution of the organolead derivative followed by a reductive elimination reaction, while the tin one was formed by a dephenylation process. Reactions in solution of the organotin derivative are complicated and depending on the working conditions different compounds could be isolated: the organostannoxane [Sn 2 Ph 4 ClO(OH)] 2 , which was confirmed by X-ray crystallography, or a complex containing a triazine-3-thione ligand, formed by the loss of one of the thiosemicarbazone arms with subsequent cyclisation. The compounds were characterized by IR, mass spectrometry, 1 H, 13 C and 119 Sn NMR spectroscopy in solution and in the solid state. The structure of [Pb(LH 4 )] has been studied by X-ray diffraction and the ligand acts as a N 2 S 2 planar bideprotonated ligand, with the lead(II) ion localized 1.3858Å over this plane.

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